HuagongsheHuagongshe Chemistry Print Report · For research reference only
Lithium Hydroxide → HCID 10455140, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Lithium Hydroxide | HCID 3939 | — |
| Reactant | HCID 68871852 | HCID 68871852 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 10455140 | HCID 10455140 | 55% |
Reaction Steps
Lithium hydroxide (3.7 mg, 0.154 mmol) in water (1 ml) was added into methyl 2-({4-[2-({[(2,4-difluorophenyl)amino]carbonyl}amino)ethyl]phenoxy}methyl)benzoate (34 mg, 0.077 mmol) dissolved in THF (2 ml). The mixture was then irradiated in a microwave oven (Smith Synthesizer) at 150° C. for 7 minutes and then evaporated to remove THF. The residue was acidified with 1% hydrochloric acid, pH˜4, and extracted with ethyl acetate (×2). The organic extracts were combined and dried with magnesium sulphate and then evaporated. Chromatography of the residue on a column (ISOLUTE® SI, 1 g/6 ml) using MeOH/DCM (1:99, 2:98, 4:96 and then 10:90) as eluant gave 18 mg the desired product, yield 55%.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07521461B2 |
| Source dataset | uspto-grants-2009_04 |
| ORD ID | ord-a1bdcb49a8654abfa905205878bb9e8a |
| Source note | uspto-grants-2009_04 |